# om020815b.cif data_mat23 #------------------------------------------------------------------------------ _audit_creation_date '2000-02-14' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; 1999-10-22 Report by acw 2002-09-24 cif by acw 2002-10-05 Organometallics code: OM020815B ; #------------------------------------------------------------------------------ _publ_requested_journal ' Organometallics' _publ_requested_category ' fm ' _publ_contact_author_name ' Anthony C. Willis ' _publ_contact_author_address ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 61 2 6249 4109 ' _publ_contact_author_fax ' 61 2 6249 0750 ' _publ_contact_author_email ' willis@rsc.anu.edu.au ' loop_ _publ_author_name _publ_author_address 'Martin A. Bennett ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; 'Matthew J. Byrnes ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; 'Anthony C. Willis ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_section_title ; (Ethene)bis(acetylacetonato) Complexes of Divalent and Trivalent Ruthenium ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (1999). maXus Computer Program for the Solution and Refinement of Crystal Structures. Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Otwinowski, Z. and Minor, W, (1997). In Methods in Enzymology, 276, edited by C.W. Carter, Jr. & R.M. Sweet pp. 307-326, New York:Academic Press. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garcia-Granda, S., Gould, R.O., Smits, J.M.M. and Smykalla, C. (1992). The DIRDIF program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. Blessing, R. H.; Acta Crystallogr., Section A, 51, 33-37 (1995). Blessing, R. H.; J. Appl. Crystallogr., 30, 421-426 (1997). ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #------------------------------------------------------------------------------ _computing_cell_refinement 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_data_collection 'KappaCCD' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution ; 'DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 7.6278(2) _cell_length_b 8.9725(4) _cell_length_c 12.5027(5) _cell_angle_alpha 76.719(2) _cell_angle_beta 74.620(2) _cell_angle_gamma 70.659(2) _cell_volume 768.96(5) _cell_formula_units_Z 2 _cell_measurement_temperature 200.0 _cell_measurement_reflns_used 7792 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 355.40 _chemical_formula_analytical ? _chemical_formula_sum 'C14 H22 O4 Ru ' _chemical_formula_moiety 'C14 H22 O4 Ru ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 364.00 _exptl_absorpt_coefficient_mu 1.027 # Absorption correction _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min .845 _exptl_absorpt_correction_T_max .905 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995) ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 200.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method ' \w scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 #loop_ #_diffrn_standard_refln_index_h #_diffrn_standard_refln_index_k #_diffrn_standard_refln_index_l # _diffrn_reflns_number 8834 _reflns_number_total 3476 _reflns_number_gt 3285 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.02824 _diffrn_reflns_av_sigmaI/netI 0.060 _diffrn_measured_fraction_theta_max .99 _diffrn_measured_fraction_theta_full .99 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.55 _diffrn_reflns_theta_full 27.55 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 28 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 44 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 8 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru 0 2 -1.420 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ru(1) 0.09943(2) 0.24041(1) 0.30288(1) 0.02297(6) 1.000 . Uani d ? O(1) 0.2754(2) 0.0409(2) 0.3838(1) 0.0278(3) 1.000 . Uani d ? O(2) 0.2990(2) 0.2199(2) 0.1542(1) 0.0312(4) 1.000 . Uani d ? O(3) 0.2634(2) 0.3667(2) 0.3277(1) 0.0292(4) 1.000 . Uani d ? O(4) -0.0413(2) 0.4268(2) 0.1979(1) 0.0300(4) 1.000 . Uani d ? C(1) 0.5493(3) -0.1658(3) 0.4153(2) 0.0354(5) 1.000 . Uani d ? C(2) 0.4446(3) -0.0289(2) 0.3391(2) 0.0270(5) 1.000 . Uani d ? C(3) 0.5399(3) 0.0103(3) 0.2296(2) 0.0336(5) 1.000 . Uani d ? C(4) 0.4675(3) 0.1296(3) 0.1463(2) 0.0323(5) 1.000 . Uani d ? C(5) 0.5969(4) 0.1588(4) 0.0342(2) 0.0508(7) 1.000 . Uani d ? C(6) 0.4048(3) 0.5727(3) 0.2916(2) 0.0418(6) 1.000 . Uani d ? C(7) 0.2591(3) 0.5062(2) 0.2740(2) 0.0300(5) 1.000 . Uani d ? C(8) 0.1385(3) 0.5989(3) 0.2015(2) 0.0340(5) 1.000 . Uani d ? C(9) 0.0035(3) 0.5572(3) 0.1662(2) 0.0319(5) 1.000 . Uani d ? C(10) -0.1015(4) 0.6742(3) 0.0806(2) 0.0471(7) 1.000 . Uani d ? C(11) -0.1250(3) 0.3800(3) 0.4238(2) 0.0311(5) 1.000 . Uani d ? C(12) -0.0274(3) 0.2436(3) 0.4833(2) 0.0333(5) 1.000 . Uani d ? C(13) -0.1308(3) 0.1377(3) 0.3099(2) 0.0409(7) 1.000 . Uani d ? C(14) 0.0263(3) 0.0676(3) 0.2379(2) 0.0381(6) 1.000 . Uani d ? H(1) 0.4692 -0.2309 0.4548 0.042 1.000 . Uiso c ? H(2) 0.6598 -0.2279 0.3716 0.042 1.000 . Uiso c ? H(3) 0.5850 -0.1251 0.4674 0.042 1.000 . Uiso c ? H(4) 0.6684 -0.0512 0.2097 0.040 1.000 . Uiso c ? H(5) 0.7200 0.0860 0.0347 0.061 1.000 . Uiso c ? H(6) 0.5477 0.1436 -0.0234 0.061 1.000 . Uiso c ? H(7) 0.6046 0.2653 0.0208 0.061 1.000 . Uiso c ? H(8) 0.5259 0.5239 0.2494 0.050 1.000 . Uiso c ? H(9) 0.4090 0.5510 0.3690 0.050 1.000 . Uiso c ? H(10) 0.3714 0.6849 0.2673 0.050 1.000 . Uiso c ? H(11) 0.1493 0.7037 0.1723 0.041 1.000 . Uiso c ? H(12) -0.0725 0.7727 0.0680 0.057 1.000 . Uiso c ? H(13) -0.0638 0.6322 0.0121 0.057 1.000 . Uiso c ? H(14) -0.2342 0.6913 0.1076 0.057 1.000 . Uiso c ? H(15) -0.095(3) 0.472(3) 0.412(2) 0.037 1.000 . Uiso d ? H(16) -0.236(4) 0.391(3) 0.409(2) 0.037 1.000 . Uiso d ? H(17) 0.078(4) 0.243(3) 0.514(2) 0.040 1.000 . Uiso d ? H(18) -0.078(4) 0.161(3) 0.512(2) 0.040 1.000 . Uiso d ? H(19) -0.218(4) 0.217(4) 0.280(2) 0.049 1.000 . Uiso d ? H(20) -0.187(4) 0.085(3) 0.389(2) 0.049 1.000 . Uiso d ? H(21) 0.050(4) 0.107(3) 0.157(2) 0.046 1.000 . Uiso d ? H(22) 0.099(4) -0.037(4) 0.263(2) 0.046 1.000 . Uiso d ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.0233(1) 0.0206(1) 0.0239(1) -0.00540(7) -0.00714(7) -0.00024(7) O(1) 0.0278(7) 0.0234(7) 0.0289(7) -0.0037(6) -0.0098(5) 0.0014(5) O(2) 0.0315(7) 0.0319(8) 0.0252(7) -0.0065(6) -0.0034(5) -0.0013(6) O(3) 0.0305(7) 0.0275(8) 0.0312(7) -0.0106(6) -0.0094(6) -0.0010(6) O(4) 0.0323(7) 0.0271(8) 0.0283(7) -0.0030(6) -0.0130(6) -0.0002(6) C(1) 0.034(1) 0.028(1) 0.043(1) -0.0012(8) -0.0166(9) -0.0062(9) C(2) 0.0266(9) 0.0215(9) 0.037(1) -0.0050(7) -0.0126(7) -0.0078(8) C(3) 0.0248(9) 0.033(1) 0.040(1) -0.0037(8) -0.0035(8) -0.0090(9) C(4) 0.032(1) 0.033(1) 0.032(1) -0.0116(9) -0.0001(8) -0.0086(9) C(5) 0.042(1) 0.058(2) 0.041(1) -0.014(1) 0.005(1) -0.002(1) C(6) 0.044(1) 0.038(1) 0.049(1) -0.021(1) -0.005(1) -0.007(1) C(7) 0.0323(9) 0.026(1) 0.029(1) -0.0102(8) 0.0018(7) -0.0071(8) C(8) 0.040(1) 0.024(1) 0.033(1) -0.0100(9) -0.0023(8) 0.0001(8) C(9) 0.036(1) 0.026(1) 0.0238(9) -0.0005(8) -0.0036(8) -0.0015(8) C(10) 0.062(1) 0.032(1) 0.037(1) 0.001(1) -0.018(1) 0.003(1) C(11) 0.028(1) 0.032(1) 0.028(1) -0.0037(8) -0.0019(7) -0.0057(8) C(12) 0.031(1) 0.038(1) 0.025(1) -0.0078(9) -0.0014(8) -0.0016(8) C(13) 0.035(1) 0.037(1) 0.059(2) -0.016(1) -0.015(1) -0.008(1) C(14) 0.045(1) 0.035(1) 0.043(1) -0.016(1) -0.014(1) -0.010(1) #------------------------------------------------------------------------------ _refine_special_details ; \s^2^(Fo) is the larger of the value from averaging of equivalent reflections or counting statistics. Hydrogen atoms of acac groups at calculated positions - those of Me groups oriented to best-fit peaks in difference electron-density map. Hydrogen atoms of ethylene groups refined xyz. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00040|Fo|^2^]' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3285 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0265 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_all 0.0356 _refine_ls_wR_factor_ref 0.0349 _refine_ls_goodness_of_fit_all 1.216 _refine_ls_goodness_of_fit_ref 1.227 _refine_ls_shift/su_max 0.0010 _refine_ls_shift/su_mean 0.0010 _refine_diff_density_min -0.96 _refine_diff_density_max 0.44 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru(1) O(1) 2.080(1) . . yes Ru(1) O(2) 2.068(1) . . yes Ru(1) O(3) 2.061(1) . . yes Ru(1) O(4) 2.055(1) . . yes Ru(1) C(11) 2.205(2) . . yes Ru(1) C(12) 2.209(2) . . yes Ru(1) C(13) 2.212(2) . . yes Ru(1) C(14) 2.183(2) . . yes O(1) C(2) 1.270(2) . . yes O(2) C(4) 1.264(2) . . yes O(3) C(7) 1.272(3) . . yes O(4) C(9) 1.273(3) . . yes C(1) C(2) 1.506(3) . . yes C(1) H(1) 0.95 . . no C(1) H(2) 0.95 . . no C(1) H(3) 0.95 . . no C(2) C(3) 1.396(3) . . yes C(3) C(4) 1.391(3) . . yes C(3) H(4) 0.95 . . no C(4) C(5) 1.509(3) . . yes C(5) H(5) 0.95 . . no C(5) H(6) 0.95 . . no C(5) H(7) 0.95 . . no C(6) C(7) 1.506(3) . . yes C(6) H(8) 0.95 . . no C(6) H(9) 0.95 . . no C(6) H(10) 0.95 . . no C(7) C(8) 1.396(3) . . yes C(8) C(9) 1.403(3) . . yes C(8) H(11) 0.95 . . no C(9) C(10) 1.507(3) . . yes C(10) H(12) 0.95 . . no C(10) H(13) 0.95 . . no C(10) H(14) 0.95 . . no C(11) C(12) 1.370(3) . . yes C(11) H(15) 0.90(3) . . no C(11) H(16) 0.89(3) . . no C(12) H(17) 0.98(2) . . no C(12) H(18) 0.90(3) . . no C(13) C(14) 1.353(4) . . yes C(13) H(19) 0.88(3) . . no C(13) H(20) 1.04(3) . . no C(14) H(21) 0.98(3) . . no C(14) H(22) 0.95(3) . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Ru(1) O(2) 90.32(6) . . . yes O(1) Ru(1) O(3) 85.87(6) . . . yes O(1) Ru(1) O(4) 170.05(5) . . . yes O(1) Ru(1) C(11) 111.64(7) . . . yes O(1) Ru(1) C(12) 75.63(7) . . . yes O(1) Ru(1) C(13) 98.47(8) . . . yes O(1) Ru(1) C(14) 85.18(8) . . . yes O(2) Ru(1) O(3) 81.56(6) . . . yes O(2) Ru(1) O(4) 79.86(6) . . . yes O(2) Ru(1) C(11) 152.77(8) . . . yes O(2) Ru(1) C(12) 160.95(8) . . . yes O(2) Ru(1) C(13) 112.26(8) . . . yes O(2) Ru(1) C(14) 79.25(8) . . . yes O(3) Ru(1) O(4) 94.21(6) . . . yes O(3) Ru(1) C(11) 84.11(7) . . . yes O(3) Ru(1) C(12) 84.60(8) . . . yes O(3) Ru(1) C(13) 165.35(8) . . . yes O(3) Ru(1) C(14) 158.74(9) . . . yes O(4) Ru(1) C(11) 78.24(7) . . . yes O(4) Ru(1) C(12) 114.29(7) . . . yes O(4) Ru(1) C(13) 83.92(8) . . . yes O(4) Ru(1) C(14) 91.35(8) . . . yes C(11) Ru(1) C(12) 36.17(8) . . . yes C(11) Ru(1) C(13) 81.28(9) . . . yes C(11) Ru(1) C(14) 117.13(9) . . . yes C(12) Ru(1) C(13) 83.0(1) . . . yes C(12) Ru(1) C(14) 111.66(9) . . . yes C(13) Ru(1) C(14) 35.85(9) . . . yes Ru(1) O(1) C(2) 124.0(1) . . . yes Ru(1) O(2) C(4) 124.4(1) . . . yes Ru(1) O(3) C(7) 121.4(1) . . . yes Ru(1) O(4) C(9) 121.6(1) . . . yes C(2) C(1) H(1) 109.5 . . . no C(2) C(1) H(2) 109.5 . . . no C(2) C(1) H(3) 109.5 . . . no H(1) C(1) H(2) 109.5 . . . no H(1) C(1) H(3) 109.5 . . . no H(2) C(1) H(3) 109.5 . . . no O(1) C(2) C(1) 114.9(2) . . . yes O(1) C(2) C(3) 126.6(2) . . . yes C(1) C(2) C(3) 118.4(2) . . . yes C(2) C(3) C(4) 127.2(2) . . . yes C(2) C(3) H(4) 116.4 . . . no C(4) C(3) H(4) 116.4 . . . no O(2) C(4) C(3) 126.4(2) . . . yes O(2) C(4) C(5) 114.5(2) . . . yes C(3) C(4) C(5) 119.1(2) . . . yes C(4) C(5) H(5) 109.5 . . . no C(4) C(5) H(6) 109.5 . . . no C(4) C(5) H(7) 109.5 . . . no H(5) C(5) H(6) 109.5 . . . no H(5) C(5) H(7) 109.4 . . . no H(6) C(5) H(7) 109.5 . . . no C(7) C(6) H(8) 109.5 . . . no C(7) C(6) H(9) 109.5 . . . no C(7) C(6) H(10) 109.5 . . . no H(8) C(6) H(9) 109.5 . . . no H(8) C(6) H(10) 109.5 . . . no H(9) C(6) H(10) 109.5 . . . no O(3) C(7) C(6) 114.3(2) . . . yes O(3) C(7) C(8) 127.2(2) . . . yes C(6) C(7) C(8) 118.5(2) . . . yes C(7) C(8) C(9) 128.3(2) . . . yes C(7) C(8) H(11) 115.8 . . . no C(9) C(8) H(11) 115.8 . . . no O(4) C(9) C(8) 126.9(2) . . . yes O(4) C(9) C(10) 114.3(2) . . . yes C(8) C(9) C(10) 118.7(2) . . . yes C(9) C(10) H(12) 109.5 . . . no C(9) C(10) H(13) 109.5 . . . no C(9) C(10) H(14) 109.5 . . . no H(12) C(10) H(13) 109.5 . . . no H(12) C(10) H(14) 109.5 . . . no H(13) C(10) H(14) 109.5 . . . no Ru(1) C(11) C(12) 72.1(1) . . . yes Ru(1) C(11) H(15) 103(2) . . . no Ru(1) C(11) H(16) 108(2) . . . no C(12) C(11) H(15) 121(2) . . . no C(12) C(11) H(16) 123(2) . . . no H(15) C(11) H(16) 115(2) . . . no Ru(1) C(12) C(11) 71.7(1) . . . yes Ru(1) C(12) H(17) 103(1) . . . no Ru(1) C(12) H(18) 110(2) . . . no C(11) C(12) H(17) 121(2) . . . no C(11) C(12) H(18) 120(2) . . . no H(17) C(12) H(18) 117(2) . . . no Ru(1) C(13) C(14) 70.9(1) . . . yes Ru(1) C(13) H(19) 105(2) . . . no Ru(1) C(13) H(20) 116(1) . . . no C(14) C(13) H(19) 117(2) . . . no C(14) C(13) H(20) 126(2) . . . no H(19) C(13) H(20) 112(2) . . . no Ru(1) C(14) C(13) 73.2(1) . . . yes Ru(1) C(14) H(21) 101(2) . . . no Ru(1) C(14) H(22) 109(2) . . . no C(13) C(14) H(21) 123(2) . . . no C(13) C(14) H(22) 118(2) . . . no H(21) C(14) H(22) 117(2) . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) C(12) 3.527(3) . 2_556 no O(2) C(10) 3.450(3) . 2_565 no O(4) C(10) 3.593(3) . 2_565 no C(3) C(13) 3.520(3) . 1_655 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Ru(1) O(1) C(2) C(1) . . . . 176.9(1) no Ru(1) O(1) C(2) C(3) . . . . -2.1(3) no Ru(1) O(2) C(4) C(3) . . . . 11.5(3) no Ru(1) O(2) C(4) C(5) . . . . -168.5(2) no Ru(1) O(3) C(7) C(6) . . . . -172.8(1) no Ru(1) O(3) C(7) C(8) . . . . 6.0(3) no Ru(1) O(4) C(9) C(8) . . . . -4.8(3) no Ru(1) O(4) C(9) C(10) . . . . 174.2(1) no O(1) Ru(1) O(2) C(4) . . . . -11.6(2) no O(1) Ru(1) O(3) C(7) . . . . 164.3(2) no O(1) Ru(1) O(4) C(9) . . . . -84.9(3) no O(1) Ru(1) C(11) C(12) . . . . -5.7(2) no O(1) Ru(1) C(12) C(11) . . . . 174.5(2) no O(1) Ru(1) C(13) C(14) . . . . -69.4(2) no O(1) Ru(1) C(14) C(13) . . . . 111.7(2) no O(1) C(2) C(3) C(4) . . . . -2.4(3) no O(2) Ru(1) O(1) C(2) . . . . 7.1(2) no O(2) Ru(1) O(3) C(7) . . . . 73.3(2) no O(2) Ru(1) O(4) C(9) . . . . -75.4(1) no O(2) Ru(1) C(11) C(12) . . . . -147.4(2) no O(2) Ru(1) C(12) C(11) . . . . 130.9(2) no O(2) Ru(1) C(13) C(14) . . . . 24.4(2) no O(2) Ru(1) C(14) C(13) . . . . -157.1(2) no O(2) C(4) C(3) C(2) . . . . -3.0(4) no O(3) Ru(1) O(1) C(2) . . . . -74.4(1) no O(3) Ru(1) O(2) C(4) . . . . 74.2(2) no O(3) Ru(1) O(4) C(9) . . . . 5.2(2) no O(3) Ru(1) C(11) C(12) . . . . -88.9(1) no O(3) Ru(1) C(12) C(11) . . . . 87.4(1) no O(3) Ru(1) C(13) C(14) . . . . -175.8(3) no O(3) Ru(1) C(14) C(13) . . . . 177.1(2) no O(3) C(7) C(8) C(9) . . . . -4.0(4) no O(4) Ru(1) O(1) C(2) . . . . 16.4(4) no O(4) Ru(1) O(2) C(4) . . . . 170.0(2) no O(4) Ru(1) O(3) C(7) . . . . -5.8(2) no O(4) Ru(1) C(11) C(12) . . . . 175.5(2) no O(4) Ru(1) C(12) C(11) . . . . -4.8(2) no O(4) Ru(1) C(13) C(14) . . . . 100.8(2) no O(4) Ru(1) C(14) C(13) . . . . -77.7(2) no O(4) C(9) C(8) C(7) . . . . 3.2(4) no C(1) C(2) C(3) C(4) . . . . 178.6(2) no C(2) O(1) Ru(1) C(11) . . . . -156.4(1) no C(2) O(1) Ru(1) C(12) . . . . -159.9(2) no C(2) O(1) Ru(1) C(13) . . . . 119.7(2) no C(2) O(1) Ru(1) C(14) . . . . 86.3(2) no C(2) C(3) C(4) C(5) . . . . 177.0(2) no C(4) O(2) Ru(1) C(11) . . . . 133.2(2) no C(4) O(2) Ru(1) C(12) . . . . 30.3(3) no C(4) O(2) Ru(1) C(13) . . . . -110.9(2) no C(4) O(2) Ru(1) C(14) . . . . -96.6(2) no C(6) C(7) C(8) C(9) . . . . 174.8(2) no C(7) O(3) Ru(1) C(11) . . . . -83.5(2) no C(7) O(3) Ru(1) C(12) . . . . -119.8(2) no C(7) O(3) Ru(1) C(13) . . . . -87.8(3) no C(7) O(3) Ru(1) C(14) . . . . 99.0(3) no C(7) C(8) C(9) C(10) . . . . -175.8(2) no C(9) O(4) Ru(1) C(11) . . . . 88.3(2) no C(9) O(4) Ru(1) C(12) . . . . 91.2(2) no C(9) O(4) Ru(1) C(13) . . . . 170.6(2) no C(9) O(4) Ru(1) C(14) . . . . -154.2(2) no C(11) Ru(1) C(13) C(14) . . . . 179.8(2) no C(11) Ru(1) C(14) C(13) . . . . -0.2(2) no C(11) C(12) Ru(1) C(13) . . . . -84.8(2) no C(11) C(12) Ru(1) C(14) . . . . -106.7(2) no C(12) Ru(1) C(13) C(14) . . . . -143.7(2) no C(12) Ru(1) C(14) C(13) . . . . 39.2(2) no C(12) C(11) Ru(1) C(13) . . . . 90.0(2) no C(12) C(11) Ru(1) C(14) . . . . 90.1(2) no #===END data_mat15 #------------------------------------------------------------------------------ _audit_creation_date '1998-10-19' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; 1998-10-19 Report by acw 2002-09-24 cif by acw ; #------------------------------------------------------------------------------ _publ_requested_journal ' Organometallics' _publ_requested_category ' fm ' _publ_contact_author_name ' Anthony C. Willis ' _publ_contact_author_address ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 61 2 6125 4109 ' _publ_contact_author_fax ' 61 2 6125 0750 ' _publ_contact_author_email ' willis@rsc.anu.edu.au ' loop_ _publ_author_name _publ_author_address 'Martin A. Bennett ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; 'Matthew J. Byrnes ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; 'Anthony C. Willis ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_section_title ; (Ethene)bis(acetylacetonato) Complexes of Divalent and Trivalent Ruthenium ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. de Meulenaer, J. & Tompa, H. (1965), Acta Cryst. 19, 1014. Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 11.869(3) _cell_length_b 10.400(4) _cell_length_c 12.247(2) _cell_angle_alpha 90 _cell_angle_beta 103.26(1) _cell_angle_gamma 90 _cell_volume 1471.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 24.9 _cell_measurement_theta_max 27.4 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'plate' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 344.37 _chemical_formula_analytical ? _chemical_formula_sum 'C12 H21 N O4 Ru ' _chemical_formula_moiety 'C12 H21 N O4 Ru ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 704.00 _exptl_absorpt_coefficient_mu 1.049 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details ; analytical (de Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_max 0.920 _exptl_absorpt_correction_T_min 0.752 _exptl_special_details ; The scan width was (1.20+0.34tan\q)\% with an \w scan speed of 4\% per minute (up to 5 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.35 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 3755 _reflns_number_total 3401 _reflns_number_gt 2713 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.01419 _diffrn_reflns_av_sigmaI/netI 0.040 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 27.55 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_max 1. _diffrn_measured_fraction_theta_full 1. _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.04354 _diffrn_orient_matrix_UB_12 0.05747 _diffrn_orient_matrix_UB_13 -0.06065 _diffrn_orient_matrix_UB_21 -0.05419 _diffrn_orient_matrix_UB_22 0.02366 _diffrn_orient_matrix_UB_23 0.04838 _diffrn_orient_matrix_UB_31 0.05158 _diffrn_orient_matrix_UB_32 0.07337 _diffrn_orient_matrix_UB_33 0.03191 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 48 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 84 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 4 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 16 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru 0 4 -1.420 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ru(1) 0.47562(1) 0.08124(2) 0.29102(1) 0.03221(5) 1.000 . Uani d ? O(1) 0.6336(1) 0.0875(2) 0.4026(1) 0.0389(4) 1.000 . Uani d ? O(2) 0.4928(1) 0.2649(2) 0.2326(1) 0.0417(4) 1.000 . Uani d ? O(3) 0.3177(1) 0.0638(2) 0.1813(1) 0.0396(4) 1.000 . Uani d ? O(4) 0.4053(1) 0.1767(2) 0.4103(1) 0.0378(4) 1.000 . Uani d ? N(1) 0.4313(2) -0.0823(2) 0.3739(2) 0.0419(6) 1.000 . Uani d ? C(1) 0.8148(3) 0.1690(4) 0.4948(2) 0.0576(9) 1.000 . Uani d ? C(2) 0.7031(2) 0.1820(2) 0.4087(2) 0.0394(6) 1.000 . Uani d ? C(3) 0.6833(2) 0.2941(3) 0.3449(2) 0.0460(7) 1.000 . Uani d ? C(4) 0.5853(2) 0.3299(2) 0.2649(2) 0.0431(7) 1.000 . Uani d ? C(5) 0.5853(3) 0.4574(3) 0.2065(3) 0.064(1) 1.000 . Uani d ? C(6) 0.1167(3) 0.0638(3) 0.1158(3) 0.0554(8) 1.000 . Uani d ? C(7) 0.2232(2) 0.0956(2) 0.2046(2) 0.0388(6) 1.000 . Uani d ? C(8) 0.2106(2) 0.1556(2) 0.3043(2) 0.0431(7) 1.000 . Uani d ? C(9) 0.2965(2) 0.1919(2) 0.3975(2) 0.0395(6) 1.000 . Uani d ? C(10) 0.2599(3) 0.2539(4) 0.4944(3) 0.0617(9) 1.000 . Uani d ? C(11) 0.5604(3) 0.0450(3) 0.1570(2) 0.0508(8) 1.000 . Uani d ? C(12) 0.5373(3) -0.0697(3) 0.1998(2) 0.0526(8) 1.000 . Uani d ? H(1) 0.826(3) 0.078(3) 0.519(2) 0.069 1.000 . Uiso d ? H(2) 0.881(3) 0.180(3) 0.466(2) 0.069 1.000 . Uiso d ? H(3) 0.815(3) 0.209(3) 0.546(2) 0.069 1.000 . Uiso d ? H(4) 0.739(2) 0.355(3) 0.366(2) 0.055 1.000 . Uiso d ? H(5) 0.613(3) 0.444(3) 0.137(3) 0.077 1.000 . Uiso d ? H(6) 0.617(3) 0.511(3) 0.247(3) 0.077 1.000 . Uiso d ? H(7) 0.513(3) 0.489(3) 0.172(3) 0.077 1.000 . Uiso d ? H(8) 0.096(3) -0.022(3) 0.109(2) 0.067 1.000 . Uiso d ? H(9) 0.124(3) 0.079(3) 0.045(2) 0.067 1.000 . Uiso d ? H(10) 0.051(3) 0.106(3) 0.120(2) 0.067 1.000 . Uiso d ? H(11) 0.139(2) 0.170(2) 0.313(2) 0.052 1.000 . Uiso d ? H(12) 0.291(3) 0.211(3) 0.556(2) 0.074 1.000 . Uiso d ? H(13) 0.188(3) 0.248(3) 0.492(2) 0.074 1.000 . Uiso d ? H(14) 0.285(3) 0.326(3) 0.504(3) 0.074 1.000 . Uiso d ? H(15) 0.491(2) -0.125(2) 0.418(2) 0.050 1.000 . Uiso d ? H(16) 0.396(2) -0.134(2) 0.337(2) 0.050 1.000 . Uiso d ? H(17) 0.392(2) -0.063(2) 0.427(2) 0.050 1.000 . Uiso d ? H(18) 0.636(3) 0.079(3) 0.174(2) 0.061 1.000 . Uiso d ? H(19) 0.507(2) 0.076(2) 0.080(2) 0.061 1.000 . Uiso d ? H(20) 0.594(3) -0.125(3) 0.247(2) 0.063 1.000 . Uiso d ? H(21) 0.472(2) -0.119(3) 0.159(2) 0.063 1.000 . Uiso d ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.02793(9) 0.0400(1) 0.02735(9) -0.00187(8) 0.00353(6) 0.00080(8) O(1) 0.0316(8) 0.0495(9) 0.0322(8) -0.0002(7) 0.0005(6) 0.0009(7) O(2) 0.0377(8) 0.046(1) 0.0401(8) -0.0015(8) 0.0066(7) 0.0081(7) O(3) 0.0326(8) 0.050(1) 0.0336(8) -0.0031(7) 0.0022(6) 0.0003(7) O(4) 0.0364(8) 0.0428(9) 0.0338(8) -0.0012(7) 0.0071(6) -0.0030(7) N(1) 0.048(1) 0.041(1) 0.034(1) -0.004(1) 0.0048(9) 0.0003(9) C(1) 0.037(1) 0.081(2) 0.048(2) -0.001(2) -0.003(1) -0.015(2) C(2) 0.030(1) 0.054(1) 0.034(1) -0.003(1) 0.0071(9) -0.008(1) C(3) 0.036(1) 0.052(2) 0.050(1) -0.014(1) 0.010(1) -0.005(1) C(4) 0.043(1) 0.046(1) 0.043(1) -0.004(1) 0.016(1) 0.001(1) C(5) 0.064(2) 0.054(2) 0.075(2) -0.006(2) 0.018(2) 0.015(2) C(6) 0.037(1) 0.066(2) 0.057(2) -0.005(1) -0.003(1) -0.003(2) C(7) 0.032(1) 0.039(1) 0.042(1) -0.003(1) 0.0015(9) 0.006(1) C(8) 0.033(1) 0.046(1) 0.051(1) 0.003(1) 0.011(1) 0.004(1) C(9) 0.044(1) 0.036(1) 0.039(1) 0.004(1) 0.012(1) 0.005(1) C(10) 0.057(2) 0.077(2) 0.055(2) 0.009(2) 0.020(1) -0.009(2) C(11) 0.052(2) 0.066(2) 0.037(1) 0.005(1) 0.018(1) -0.002(1) C(12) 0.050(2) 0.058(2) 0.054(2) 0.003(1) 0.020(1) -0.011(1) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]' _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2713 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0209 _refine_ls_wR_factor_all 0.0244 _refine_ls_wR_factor_ref 0.0223 _refine_ls_goodness_of_fit_all 1.294 _refine_ls_goodness_of_fit_ref 1.333 _refine_ls_shift/su_max 0.0480 _refine_ls_shift/su_mean 0.0060 _refine_diff_density_min -0.30 _refine_diff_density_max 0.28 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru(1) O(1) 2.052(2) . . yes Ru(1) O(2) 2.066(2) . . yes Ru(1) O(3) 2.048(2) . . yes Ru(1) O(4) 2.092(2) . . yes Ru(1) N(1) 2.108(2) . . yes Ru(1) C(11) 2.147(3) . . yes Ru(1) C(12) 2.151(3) . . yes O(1) C(2) 1.275(3) . . yes O(2) C(4) 1.272(3) . . yes O(3) C(7) 1.264(3) . . yes O(4) C(9) 1.275(3) . . yes N(1) H(15) 0.90(3) . . no N(1) H(16) 0.77(2) . . no N(1) H(17) 0.91(3) . . no C(1) C(2) 1.499(3) . . yes C(1) H(1) 1.00(3) . . no C(1) H(2) 0.93(3) . . no C(1) H(3) 0.75(3) . . no C(2) C(3) 1.393(4) . . yes C(3) C(4) 1.389(3) . . yes C(3) H(4) 0.91(3) . . no C(4) C(5) 1.507(4) . . yes C(5) H(5) 0.99(3) . . no C(5) H(6) 0.79(3) . . no C(5) H(7) 0.92(3) . . no C(6) C(7) 1.503(3) . . yes C(6) H(8) 0.93(3) . . no C(6) H(9) 0.91(3) . . no C(6) H(10) 0.91(3) . . no C(7) C(8) 1.409(3) . . yes C(8) C(9) 1.396(3) . . yes C(8) H(11) 0.90(2) . . no C(9) C(10) 1.500(4) . . yes C(10) H(12) 0.88(3) . . no C(10) H(13) 0.85(3) . . no C(10) H(14) 0.81(3) . . no C(11) C(12) 1.356(4) . . yes C(11) H(18) 0.94(3) . . no C(11) H(19) 1.06(3) . . no C(12) H(20) 0.96(3) . . no C(12) H(21) 0.97(3) . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Ru(1) O(2) 93.07(6) . . . yes O(1) Ru(1) O(3) 176.67(6) . . . yes O(1) Ru(1) O(4) 88.28(6) . . . yes O(1) Ru(1) N(1) 89.74(8) . . . yes O(1) Ru(1) C(11) 89.87(9) . . . yes O(1) Ru(1) C(12) 90.05(9) . . . yes O(2) Ru(1) O(3) 90.18(6) . . . yes O(2) Ru(1) O(4) 83.68(6) . . . yes O(2) Ru(1) N(1) 165.43(8) . . . yes O(2) Ru(1) C(11) 78.30(9) . . . yes O(2) Ru(1) C(12) 115.02(9) . . . yes O(3) Ru(1) O(4) 92.79(6) . . . yes O(3) Ru(1) N(1) 87.29(7) . . . yes O(3) Ru(1) C(11) 90.09(9) . . . yes O(3) Ru(1) C(12) 87.93(9) . . . yes O(4) Ru(1) N(1) 82.12(8) . . . yes O(4) Ru(1) C(11) 161.75(9) . . . yes O(4) Ru(1) C(12) 161.29(9) . . . yes N(1) Ru(1) C(11) 116.0(1) . . . yes N(1) Ru(1) C(12) 79.2(1) . . . yes C(11) Ru(1) C(12) 36.8(1) . . . yes Ru(1) O(1) C(2) 122.9(1) . . . yes Ru(1) O(2) C(4) 122.0(2) . . . yes Ru(1) O(3) C(7) 123.7(1) . . . yes Ru(1) O(4) C(9) 121.9(1) . . . yes Ru(1) N(1) H(15) 116(2) . . . no Ru(1) N(1) H(16) 117(2) . . . no Ru(1) N(1) H(17) 113(2) . . . no H(15) N(1) H(16) 105(3) . . . no H(15) N(1) H(17) 98(2) . . . no H(16) N(1) H(17) 106(3) . . . no C(2) C(1) H(1) 109(2) . . . no C(2) C(1) H(2) 114(2) . . . no C(2) C(1) H(3) 112(2) . . . no H(1) C(1) H(2) 99(3) . . . no H(1) C(1) H(3) 108(3) . . . no H(2) C(1) H(3) 113(3) . . . no O(1) C(2) C(1) 115.3(2) . . . yes O(1) C(2) C(3) 126.1(2) . . . yes C(1) C(2) C(3) 118.6(2) . . . yes C(2) C(3) C(4) 128.8(2) . . . yes C(2) C(3) H(4) 114(2) . . . no C(4) C(3) H(4) 117(2) . . . no O(2) C(4) C(3) 126.9(2) . . . yes O(2) C(4) C(5) 114.5(2) . . . yes C(3) C(4) C(5) 118.6(2) . . . yes C(4) C(5) H(5) 109(2) . . . no C(4) C(5) H(6) 112(3) . . . no C(4) C(5) H(7) 115(2) . . . no H(5) C(5) H(6) 116(3) . . . no H(5) C(5) H(7) 97(3) . . . no H(6) C(5) H(7) 107(3) . . . no C(7) C(6) H(8) 116(2) . . . no C(7) C(6) H(9) 114(2) . . . no C(7) C(6) H(10) 117(2) . . . no H(8) C(6) H(9) 100(3) . . . no H(8) C(6) H(10) 105(3) . . . no H(9) C(6) H(10) 104(3) . . . no O(3) C(7) C(6) 114.9(2) . . . yes O(3) C(7) C(8) 126.0(2) . . . yes C(6) C(7) C(8) 119.1(2) . . . yes C(7) C(8) C(9) 128.7(2) . . . yes C(7) C(8) H(11) 118(2) . . . no C(9) C(8) H(11) 113(2) . . . no O(4) C(9) C(8) 126.6(2) . . . yes O(4) C(9) C(10) 115.2(2) . . . yes C(8) C(9) C(10) 118.3(2) . . . yes C(9) C(10) H(12) 109(2) . . . no C(9) C(10) H(13) 114(2) . . . no C(9) C(10) H(14) 110(2) . . . no H(12) C(10) H(13) 102(3) . . . no H(12) C(10) H(14) 106(3) . . . no H(13) C(10) H(14) 114(3) . . . no Ru(1) C(11) C(12) 71.8(2) . . . yes Ru(1) C(11) H(18) 110(2) . . . no Ru(1) C(11) H(19) 110(2) . . . no C(12) C(11) H(18) 121(2) . . . no C(12) C(11) H(19) 119(1) . . . no H(18) C(11) H(19) 115(2) . . . no Ru(1) C(12) C(11) 71.4(2) . . . yes Ru(1) C(12) H(20) 113(2) . . . no Ru(1) C(12) H(21) 109(2) . . . no C(11) C(12) H(20) 125(2) . . . no C(11) C(12) H(21) 118(2) . . . no H(20) C(12) H(21) 111(3) . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) N(1) 3.009(3) . 3_656 no O(2) C(1) 3.256(3) . 4_454 no O(3) C(1) 3.593(4) . 4_454 no O(4) N(1) 3.059(3) . 3_656 no N(1) C(2) 3.558(3) . 3_656 no N(1) N(1) 3.580(4) . 3_656 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Ru(1) O(1) C(2) C(1) . . . . -179.6(2) no Ru(1) O(1) C(2) C(3) . . . . 1.5(3) no Ru(1) O(2) C(4) C(3) . . . . -3.6(3) no Ru(1) O(2) C(4) C(5) . . . . 175.4(2) no Ru(1) O(3) C(7) C(6) . . . . -174.8(2) no Ru(1) O(3) C(7) C(8) . . . . 4.8(3) no Ru(1) O(4) C(9) C(8) . . . . -3.4(3) no Ru(1) O(4) C(9) C(10) . . . . 175.8(2) no O(1) Ru(1) O(2) C(4) . . . . 5.1(2) no O(1) Ru(1) O(3) C(7) . . . . 103(1) no O(1) Ru(1) O(4) C(9) . . . . -171.4(2) no O(1) Ru(1) C(11) C(12) . . . . 90.2(2) no O(1) Ru(1) C(12) C(11) . . . . -89.7(2) no O(1) C(2) C(3) C(4) . . . . 2.1(4) no O(2) Ru(1) O(1) C(2) . . . . -4.1(2) no O(2) Ru(1) O(3) C(7) . . . . -89.8(2) no O(2) Ru(1) O(4) C(9) . . . . 95.3(2) no O(2) Ru(1) C(11) C(12) . . . . -176.6(2) no O(2) Ru(1) C(12) C(11) . . . . 3.7(2) no O(2) C(4) C(3) C(2) . . . . -0.9(5) no O(3) Ru(1) O(1) C(2) . . . . 163(1) no O(3) Ru(1) O(2) C(4) . . . . -174.2(2) no O(3) Ru(1) O(4) C(9) . . . . 5.4(2) no O(3) Ru(1) C(11) C(12) . . . . -86.4(2) no O(3) Ru(1) C(12) C(11) . . . . 92.9(2) no O(3) C(7) C(8) C(9) . . . . -0.4(4) no O(4) Ru(1) O(1) C(2) . . . . -87.7(2) no O(4) Ru(1) O(2) C(4) . . . . 93.0(2) no O(4) Ru(1) O(3) C(7) . . . . -6.2(2) no O(4) Ru(1) C(11) C(12) . . . . 174.4(2) no O(4) Ru(1) C(12) C(11) . . . . -174.5(2) no O(4) C(9) C(8) C(7) . . . . -0.3(4) no N(1) Ru(1) O(1) C(2) . . . . -169.8(2) no N(1) Ru(1) O(2) C(4) . . . . 105.9(3) no N(1) Ru(1) O(3) C(7) . . . . 75.8(2) no N(1) Ru(1) O(4) C(9) . . . . -81.4(2) no N(1) Ru(1) C(11) C(12) . . . . 0.6(2) no N(1) Ru(1) C(12) C(11) . . . . -179.5(2) no C(1) C(2) C(3) C(4) . . . . -176.7(3) no C(2) O(1) Ru(1) C(11) . . . . 74.2(2) no C(2) O(1) Ru(1) C(12) . . . . 111.0(2) no C(2) C(3) C(4) C(5) . . . . -179.8(3) no C(4) O(2) Ru(1) C(11) . . . . -84.2(2) no C(4) O(2) Ru(1) C(12) . . . . -86.4(2) no C(6) C(7) C(8) C(9) . . . . 179.1(3) no C(7) O(3) Ru(1) C(11) . . . . -168.1(2) no C(7) O(3) Ru(1) C(12) . . . . 155.1(2) no C(7) C(8) C(9) C(10) . . . . -179.5(3) no C(9) O(4) Ru(1) C(11) . . . . 104.2(3) no C(9) O(4) Ru(1) C(12) . . . . -86.4(3) no #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_D _geom_bond_atom_site_label_H _geom_contact_atom_site_label_A _geom_bond_distance_DH _geom_contact_distance_HA _geom_contact_distance_DA _geom_angle_DHA _geom_contact_site_symmetry_A 'N(1)' 'H(15)' 'O(4)' '0.90(3)' '2.24(3)' '2.759(3)' '150(2)' '3_656' 'N(1)' 'H(17)' 'O(1)' '0.91(3)' '2.19(3)' '2.935(3)' '150(2)' '3_656' 'N(1)' 'H(17)' 'O(3)' '0.91(3)' '3.22(3)' '2.869(3)' '120.5(8)' '.' #===END data_mat19 #------------------------------------------------------------------------------ _audit_creation_date '1999-10-22' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; 1999-10-22 Report by acw 2002-09-24 cif by acw ; #------------------------------------------------------------------------------ _publ_requested_journal ' Organometallics' _publ_requested_category ' fm ' _publ_contact_author_name ' Anthony C. Willis ' _publ_contact_author_address ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 61 2 6249 4109 ' _publ_contact_author_fax ' 61 2 6249 0750 ' _publ_contact_author_email ' willis@rsc.anu.edu.au ' loop_ _publ_author_name _publ_author_address 'Martin A. Bennett ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; 'Matthew J. Byrnes ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; 'Anthony C. Willis ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_section_title ; (Ethene)bis(acetylacetonato) Complexes of Divalent and Trivalent Ruthenium ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. de Meulenaer, J. & Tompa, H. (1965), Acta Cryst. 19, 1014. Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 8.340(1) _cell_length_b 17.307(1) _cell_length_c 13.026(1) _cell_angle_alpha 90 _cell_angle_beta 99.324(9) _cell_angle_gamma 90 _cell_volume 1855.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 243.2 _cell_measurement_reflns_used 23 _cell_measurement_theta_min 54.6 _cell_measurement_theta_max 54.9 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'plate' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 406.44 _chemical_formula_analytical ? _chemical_formula_sum 'C17 H23 N O4 Ru ' _chemical_formula_moiety 'C17 H23 N O4 Ru ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 832.00 _exptl_absorpt_coefficient_mu 7.142 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details ; analytical (de Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_max 0.580 _exptl_absorpt_correction_T_min 0.279 _exptl_special_details ; The scan width was (1.20+0.30tan\q)\% with an \w scan speed of 16\% per minute (up to 5 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. Data can only be collected to 2theta 120 deg on a AFC6R diffractometer when the evacuated beam tunnel in used. Mass attenuation coefficients for absorption from International Tables for X-ray Crystallography, Vol IV (1974) Table 2.1C. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 243.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC6R' _diffrn_measurement_device_details ; Rigaku AFC6R diffractometer with extended arm and evacuated collimator and beam tunnel. Data cannot be collected beyond \y 60 deg in this configuration. ; _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.10 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 5970 _reflns_number_total 2761 _reflns_number_gt 2551 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.04408 _diffrn_reflns_av_sigmaI/netI 0.030 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 60.06 _diffrn_reflns_theta_full 60 _diffrn_measured_fraction_theta_max 1. _diffrn_measured_fraction_theta_full 1. _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.07960 _diffrn_orient_matrix_UB_12 -0.00846 _diffrn_orient_matrix_UB_13 -0.04865 _diffrn_orient_matrix_UB_21 0.00356 _diffrn_orient_matrix_UB_22 0.05693 _diffrn_orient_matrix_UB_23 -0.01258 _diffrn_orient_matrix_UB_31 0.09174 _diffrn_orient_matrix_UB_32 0.00513 _diffrn_orient_matrix_UB_33 0.05939 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 68 0.017 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 92 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 4 0.029 0.018 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 16 0.047 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru 0 4 -0.105 3.296 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ru(1) 0.07910(2) 0.40284(1) 0.24429(1) 0.03644(6) 1.000 . Uani d ? O(1) 0.0050(2) 0.4183(1) 0.3857(1) 0.0517(5) 1.000 . Uani d ? O(2) -0.0955(2) 0.3218(1) 0.1960(1) 0.0505(5) 1.000 . Uani d ? O(3) 0.1812(2) 0.3726(1) 0.1159(1) 0.0414(4) 1.000 . Uani d ? O(4) 0.2626(2) 0.4785(1) 0.2985(1) 0.0467(5) 1.000 . Uani d ? N(1) 0.2215(2) 0.3142(1) 0.3214(1) 0.0384(5) 1.000 . Uani d ? C(1) -0.1431(4) 0.3979(2) 0.5211(3) 0.081(1) 1.000 . Uani d ? C(2) -0.1133(3) 0.3817(2) 0.4115(2) 0.0546(8) 1.000 . Uani d ? C(3) -0.2131(3) 0.3288(2) 0.3499(2) 0.0555(8) 1.000 . Uani d ? C(4) -0.2011(3) 0.3025(2) 0.2507(2) 0.0548(8) 1.000 . Uani d ? C(5) -0.3211(4) 0.2433(2) 0.2009(2) 0.086(1) 1.000 . Uani d ? C(6) 0.3717(3) 0.3713(2) 0.0006(2) 0.0621(9) 1.000 . Uani d ? C(7) 0.3149(3) 0.4007(1) 0.0984(2) 0.0437(7) 1.000 . Uani d ? C(8) 0.4094(3) 0.4557(2) 0.1590(2) 0.0516(8) 1.000 . Uani d ? C(9) 0.3838(3) 0.4894(2) 0.2515(2) 0.0492(7) 1.000 . Uani d ? C(10) 0.5101(3) 0.5447(2) 0.3063(3) 0.075(1) 1.000 . Uani d ? C(13) 0.2284(3) 0.2444(1) 0.2782(2) 0.0483(7) 1.000 . Uani d ? C(14) 0.3155(3) 0.1838(2) 0.3277(2) 0.0629(8) 1.000 . Uani d ? C(15) 0.4007(3) 0.1951(2) 0.4254(2) 0.0627(8) 1.000 . Uani d ? C(16) 0.3967(3) 0.2659(2) 0.4702(2) 0.0592(8) 1.000 . Uani d ? C(17) 0.3081(3) 0.3243(2) 0.4168(2) 0.0503(7) 1.000 . Uani d ? C(110) -0.0313(6) 0.4848(2) 0.1277(4) 0.052(1) 0.735(6) PPP Uani d ? C(111) -0.012(2) 0.5103(5) 0.173(1) 0.054 0.265 PD Uiso d ? C(120) -0.0912(5) 0.4989(3) 0.2160(3) 0.055(1) 0.735 P Uani d ? C(121) -0.133(1) 0.4549(7) 0.1502(8) 0.054 0.265 PD Uiso d ? H(1) 0.041(3) 0.513(2) 0.116(2) 0.066 1.000 . Uiso d ? H(2) -0.134(3) 0.442(2) 0.081(2) 0.066 1.000 . Uiso d ? H(3) -0.042(3) 0.532(2) 0.261(2) 0.066 1.000 . Uiso d ? H(4) -0.186(3) 0.470(2) 0.226(2) 0.066 1.000 . Uiso d ? H(5) -0.2097 0.4425 0.5209 0.097 1.000 . Uiso c ? H(6) -0.1960 0.3549 0.5460 0.097 1.000 . Uiso c ? H(7) -0.0422 0.4066 0.5650 0.097 1.000 . Uiso c ? H(8) -0.3006 0.3083 0.3799 0.067 1.000 . Uiso c ? H(9) -0.4250 0.2538 0.2186 0.104 1.000 . Uiso c ? H(10) -0.3274 0.2454 0.1274 0.104 1.000 . Uiso c ? H(11) -0.2867 0.1932 0.2251 0.104 1.000 . Uiso c ? H(12) 0.3028 0.3910 -0.0588 0.075 1.000 . Uiso c ? H(13) 0.3678 0.3164 -0.0004 0.075 1.000 . Uiso c ? H(14) 0.4800 0.3880 -0.0001 0.075 1.000 . Uiso c ? H(15) 0.5040 0.4723 0.1333 0.062 1.000 . Uiso c ? H(16) 0.4582 0.5835 0.3407 0.090 1.000 . Uiso c ? H(17) 0.5665 0.5682 0.2566 0.090 1.000 . Uiso c ? H(18) 0.5850 0.5172 0.3558 0.090 1.000 . Uiso c ? H(19) 0.1703 0.2363 0.2101 0.058 1.000 . Uiso c ? H(20) 0.3165 0.1350 0.2945 0.075 1.000 . Uiso c ? H(21) 0.4616 0.1541 0.4614 0.075 1.000 . Uiso c ? H(22) 0.4549 0.2750 0.5380 0.071 1.000 . Uiso c ? H(23) 0.3080 0.3737 0.4485 0.060 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.0354(1) 0.0384(1) 0.0359(1) 0.00036(8) 0.00671(8) 0.00002(7) O(1) 0.062(1) 0.050(1) 0.0477(9) -0.0034(9) 0.0246(8) -0.0068(9) O(2) 0.039(1) 0.067(1) 0.0455(9) -0.0133(9) 0.0052(7) -0.0042(9) O(3) 0.0425(9) 0.0457(9) 0.0366(8) -0.0041(9) 0.0081(7) -0.0018(8) O(4) 0.0409(9) 0.048(1) 0.050(1) -0.0032(8) 0.0051(7) -0.0141(9) N(1) 0.040(1) 0.043(1) 0.0321(9) 0.000(1) 0.0045(8) 0.0019(8) C(1) 0.113(3) 0.073(2) 0.071(2) -0.009(2) 0.057(2) -0.013(2) C(2) 0.067(2) 0.050(1) 0.053(1) 0.008(1) 0.029(1) 0.005(1) C(3) 0.049(2) 0.061(2) 0.062(1) -0.004(1) 0.029(1) 0.006(1) C(4) 0.043(1) 0.069(2) 0.053(1) -0.005(1) 0.007(1) 0.008(1) C(5) 0.060(2) 0.115(3) 0.085(2) -0.045(2) 0.014(2) -0.010(2) C(6) 0.060(2) 0.078(2) 0.053(2) -0.003(2) 0.021(1) -0.007(2) C(7) 0.044(1) 0.047(1) 0.041(1) 0.006(1) 0.012(1) 0.006(1) C(8) 0.037(1) 0.056(2) 0.065(2) -0.007(1) 0.017(1) -0.005(1) C(9) 0.037(1) 0.051(2) 0.059(1) 0.005(1) 0.005(1) -0.003(1) C(10) 0.044(2) 0.074(2) 0.107(2) -0.012(2) 0.010(2) -0.035(2) C(13) 0.049(2) 0.044(1) 0.050(1) -0.002(1) 0.002(1) 0.000(1) C(14) 0.062(2) 0.043(1) 0.080(2) 0.005(1) -0.001(1) 0.008(1) C(15) 0.053(2) 0.058(1) 0.074(2) 0.001(2) 0.000(1) 0.027(1) C(16) 0.056(2) 0.074(2) 0.043(1) 0.002(2) -0.004(1) 0.012(1) C(17) 0.055(2) 0.058(2) 0.036(1) -0.001(1) 0.002(1) -0.002(1) C(110) 0.054(3) 0.040(2) 0.061(2) 0.008(2) 0.004(2) 0.014(2) C(120) 0.050(2) 0.049(2) 0.067(2) 0.017(2) 0.009(2) 0.007(2) #------------------------------------------------------------------------------ _refine_special_details ; The structure was solved by direct methods and expanded using Fourier techniques. The ethylene group was found to be disordered over two orientations approximately at right angles to each other. The relative populations of the two orientations were refined. Restraints were imposed on Ru--C distances of the minor orientation to keep them near-equal. These atoms were refined with isotropic displacement factors fixed at the average value of B~eq~ of the other two ethylene sites; all other non-hydrogen atoms were refined anisotropically. Hydrogen atoms except on ethylene were included at geometrically determined positions (methyl groups aligned to best-fit peaks in difference electron density maps) which were periodically recalculated but were not refined. Four peaks were observed close to the ethylene C atoms, which appear to correspond to the hydrogen atoms of the ethylene groups. The expected hydrogen atom sites for the two orientations of the ethylene are close to being coincident. These four peaks were therefore incorporated in the structure as hydrogen atoms of full occupancy, and refined positionally. Note that distances and angles involving them are not reliable as each is, at best, a weighted average of two sites. The biggest features in the final difference Fourier were located close to the Ru atom. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2551 _refine_ls_number_parameters 227 _refine_ls_number_restraints 2 _refine_ls_number_constraints 3 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_all 0.0311 _refine_ls_wR_factor_ref 0.0307 _refine_ls_goodness_of_fit_all 1.773 _refine_ls_goodness_of_fit_ref 1.829 _refine_ls_shift/su_max 0.0160 _refine_ls_shift/su_mean 0.0060 _refine_diff_density_min -0.58 _refine_diff_density_max 0.71 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru(1) O(1) 2.054(2) . . yes Ru(1) O(2) 2.046(2) . . yes Ru(1) O(3) 2.063(2) . . yes Ru(1) O(4) 2.051(2) . . yes Ru(1) N(1) 2.095(3) . . yes Ru(1) C(110) 2.171(5) . . yes Ru(1) C(111) 2.164(8) . . yes Ru(1) C(120) 2.179(5) . . yes Ru(1) C(121) 2.179(7) . . yes O(1) C(2) 1.262(4) . . yes O(2) C(4) 1.265(4) . . yes O(3) C(7) 1.270(4) . . yes O(4) C(9) 1.278(4) . . yes N(1) C(13) 1.337(4) . . yes N(1) C(17) 1.344(4) . . yes C(1) C(2) 1.514(5) . . yes C(1) H(5) 0.95 . . no C(1) H(6) 0.95 . . no C(1) H(7) 0.95 . . no C(2) C(3) 1.399(5) . . yes C(3) C(4) 1.389(5) . . yes C(3) H(8) 0.95 . . no C(4) C(5) 1.505(5) . . yes C(5) H(9) 0.95 . . no C(5) H(10) 0.95 . . no C(5) H(11) 0.95 . . no C(6) C(7) 1.516(5) . . yes C(6) H(12) 0.95 . . no C(6) H(13) 0.95 . . no C(6) H(14) 0.95 . . no C(7) C(8) 1.396(5) . . yes C(8) C(9) 1.387(4) . . yes C(8) H(15) 0.95 . . no C(9) C(10) 1.514(5) . . yes C(10) H(16) 0.95 . . no C(10) H(17) 0.95 . . no C(10) H(18) 0.95 . . no C(13) C(14) 1.375(5) . . yes C(13) H(19) 0.95 . . no C(14) C(15) 1.367(5) . . yes C(14) H(20) 0.95 . . no C(15) C(16) 1.361(5) . . yes C(15) H(21) 0.95 . . no C(16) C(17) 1.372(5) . . yes C(16) H(22) 0.95 . . no C(17) H(23) 0.95 . . no C(110) C(120) 1.35(1) . . yes C(110) H(1) 0.81(4) . . no C(110) H(2) 1.21(4) . . no C(111) C(121) 1.39(3) . . yes C(111) H(1) 0.92(4) . . no C(111) H(3) 1.27(3) . . no C(120) H(3) 0.87(4) . . no C(120) H(4) 0.96(4) . . no C(121) H(2) 0.92(3) . . no C(121) H(4) 1.17(3) . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Ru(1) O(2) 93.58(9) . . . yes O(1) Ru(1) O(3) 169.72(9) . . . yes O(1) Ru(1) O(4) 85.65(9) . . . yes O(1) Ru(1) N(1) 83.96(9) . . . yes O(1) Ru(1) C(110) 112.8(2) . . . yes O(1) Ru(1) C(111) 98.0(5) . . . yes O(1) Ru(1) C(120) 76.7(2) . . . yes O(1) Ru(1) C(121) 96.6(4) . . . yes O(2) Ru(1) O(3) 86.76(8) . . . yes O(2) Ru(1) O(4) 176.22(9) . . . yes O(2) Ru(1) N(1) 88.0(1) . . . yes O(2) Ru(1) C(110) 91.9(2) . . . yes O(2) Ru(1) C(111) 105.8(5) . . . yes O(2) Ru(1) C(120) 93.4(2) . . . yes O(2) Ru(1) C(121) 68.7(5) . . . yes O(3) Ru(1) O(4) 93.34(8) . . . yes O(3) Ru(1) N(1) 85.78(9) . . . yes O(3) Ru(1) C(110) 77.4(2) . . . yes O(3) Ru(1) C(111) 91.8(5) . . . yes O(3) Ru(1) C(120) 113.6(2) . . . yes O(3) Ru(1) C(121) 93.1(4) . . . yes O(4) Ru(1) N(1) 88.2(1) . . . yes O(4) Ru(1) C(110) 91.8(2) . . . yes O(4) Ru(1) C(111) 77.9(5) . . . yes O(4) Ru(1) C(120) 90.0(2) . . . yes O(4) Ru(1) C(121) 115.1(5) . . . yes N(1) Ru(1) C(110) 163.2(2) . . . yes N(1) Ru(1) C(111) 165.8(5) . . . yes N(1) Ru(1) C(120) 160.6(2) . . . yes N(1) Ru(1) C(121) 156.7(5) . . . yes C(110) Ru(1) C(111) 19.3(4) . . . yes C(110) Ru(1) C(120) 36.1(3) . . . yes C(110) Ru(1) C(121) 28.7(4) . . . yes C(111) Ru(1) C(120) 25.4(5) . . . yes C(111) Ru(1) C(121) 37.3(7) . . . yes C(120) Ru(1) C(121) 30.8(4) . . . yes Ru(1) O(1) C(2) 122.4(2) . . . yes Ru(1) O(2) C(4) 122.2(2) . . . yes Ru(1) O(3) C(7) 122.6(2) . . . yes Ru(1) O(4) C(9) 122.2(2) . . . yes Ru(1) N(1) C(13) 121.3(2) . . . yes Ru(1) N(1) C(17) 121.7(2) . . . yes C(13) N(1) C(17) 117.0(3) . . . yes C(2) C(1) H(5) 109.5 . . . no C(2) C(1) H(6) 109.5 . . . no C(2) C(1) H(7) 109.5 . . . no H(5) C(1) H(6) 109.5 . . . no H(5) C(1) H(7) 109.5 . . . no H(6) C(1) H(7) 109.5 . . . no O(1) C(2) C(1) 114.3(4) . . . yes O(1) C(2) C(3) 126.4(3) . . . yes C(1) C(2) C(3) 119.2(3) . . . yes C(2) C(3) C(4) 128.4(3) . . . yes C(2) C(3) H(8) 115.8 . . . no C(4) C(3) H(8) 115.8 . . . no O(2) C(4) C(3) 126.9(4) . . . yes O(2) C(4) C(5) 114.3(3) . . . yes C(3) C(4) C(5) 118.8(3) . . . yes C(4) C(5) H(9) 109.5 . . . no C(4) C(5) H(10) 109.5 . . . no C(4) C(5) H(11) 109.5 . . . no H(9) C(5) H(10) 109.5 . . . no H(9) C(5) H(11) 109.5 . . . no H(10) C(5) H(11) 109.5 . . . no C(7) C(6) H(12) 109.5 . . . no C(7) C(6) H(13) 109.5 . . . no C(7) C(6) H(14) 109.5 . . . no H(12) C(6) H(13) 109.5 . . . no H(12) C(6) H(14) 109.5 . . . no H(13) C(6) H(14) 109.5 . . . no O(3) C(7) C(6) 115.2(3) . . . yes O(3) C(7) C(8) 126.2(3) . . . yes C(6) C(7) C(8) 118.6(3) . . . yes C(7) C(8) C(9) 128.8(3) . . . yes C(7) C(8) H(15) 115.6 . . . no C(9) C(8) H(15) 115.6 . . . no O(4) C(9) C(8) 126.8(3) . . . yes O(4) C(9) C(10) 114.4(3) . . . yes C(8) C(9) C(10) 118.8(3) . . . yes C(9) C(10) H(16) 109.5 . . . no C(9) C(10) H(17) 109.5 . . . no C(9) C(10) H(18) 109.5 . . . no H(16) C(10) H(17) 109.5 . . . no H(16) C(10) H(18) 109.5 . . . no H(17) C(10) H(18) 109.5 . . . no N(1) C(13) C(14) 123.1(3) . . . yes N(1) C(13) H(19) 118.4 . . . no C(14) C(13) H(19) 118.4 . . . no C(13) C(14) C(15) 118.9(4) . . . yes C(13) C(14) H(20) 120.5 . . . no C(15) C(14) H(20) 120.5 . . . no C(14) C(15) C(16) 118.8(3) . . . yes C(14) C(15) H(21) 120.6 . . . no C(16) C(15) H(21) 120.6 . . . no C(15) C(16) C(17) 119.7(3) . . . yes C(15) C(16) H(22) 120.2 . . . no C(17) C(16) H(22) 120.2 . . . no N(1) C(17) C(16) 122.5(3) . . . yes N(1) C(17) H(23) 118.8 . . . no C(16) C(17) H(23) 118.8 . . . no Ru(1) C(110) C(120) 72.3(3) . . . yes Ru(1) C(110) H(1) 106(3) . . . no Ru(1) C(110) H(2) 98(2) . . . no C(120) C(110) H(1) 116(3) . . . no C(120) C(110) H(2) 102(2) . . . no H(1) C(110) H(2) 139(3) . . . no Ru(1) C(111) C(121) 72.0(6) . . . yes Ru(1) C(111) H(1) 102(3) . . . no Ru(1) C(111) H(3) 88(2) . . . no C(121) C(111) H(1) 107(3) . . . no C(121) C(111) H(3) 99(2) . . . no H(1) C(111) H(3) 154(4) . . . no Ru(1) C(120) C(110) 71.6(3) . . . yes Ru(1) C(120) H(3) 99(3) . . . no Ru(1) C(120) H(4) 96(2) . . . no C(110) C(120) H(3) 119(3) . . . no C(110) C(120) H(4) 116(2) . . . no H(3) C(120) H(4) 125(3) . . . no Ru(1) C(121) C(111) 70.7(5) . . . yes Ru(1) C(121) H(2) 109(2) . . . no Ru(1) C(121) H(4) 90(2) . . . no C(111) C(121) H(2) 105(3) . . . no C(111) C(121) H(4) 92(2) . . . no H(2) C(121) H(4) 158(3) . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) C(1) 3.531(5) . 3_566 no O(2) C(16) 3.301(4) . 4_454 no O(2) C(15) 3.531(4) . 4_454 no O(3) C(15) 3.335(4) . 4_454 no O(4) C(1) 3.442(4) . 3_566 no C(14) C(111) 3.42(2) . 2_545 no C(110) C(110) 3.49(1) . 3_565 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Ru(1) O(1) C(2) C(1) . . . . 176.8(3) no Ru(1) O(1) C(2) C(3) . . . . -2.2(5) no Ru(1) O(2) C(4) C(3) . . . . -2.7(6) no Ru(1) O(2) C(4) C(5) . . . . 178.8(3) no Ru(1) O(3) C(7) C(6) . . . . 179.6(2) no Ru(1) O(3) C(7) C(8) . . . . -1.6(5) no Ru(1) O(4) C(9) C(8) . . . . 1.9(5) no Ru(1) O(4) C(9) C(10) . . . . -177.4(2) no Ru(1) N(1) C(13) C(14) . . . . -177.6(3) no Ru(1) N(1) C(17) C(16) . . . . 177.3(3) no O(1) Ru(1) O(2) C(4) . . . . 2.5(3) no O(1) Ru(1) O(3) C(7) . . . . -83.3(5) no O(1) Ru(1) O(4) C(9) . . . . 168.9(3) no O(1) Ru(1) N(1) C(13) . . . . 133.9(3) no O(1) Ru(1) N(1) C(17) . . . . -45.2(3) no O(1) Ru(1) C(110) C(120) . . . . -1.5(5) no O(1) Ru(1) C(111) C(121) . . . . -90(1) no O(1) Ru(1) C(120) C(110) . . . . 178.6(5) no O(1) Ru(1) C(121) C(111) . . . . 95(1) no O(1) C(2) C(3) C(4) . . . . 3.1(7) no O(2) Ru(1) O(1) C(2) . . . . -0.2(3) no O(2) Ru(1) O(3) C(7) . . . . -175.5(3) no O(2) Ru(1) O(4) C(9) . . . . 91(1) no O(2) Ru(1) N(1) C(13) . . . . 40.1(3) no O(2) Ru(1) N(1) C(17) . . . . -139.0(3) no O(2) Ru(1) C(110) C(120) . . . . 93.2(4) no O(2) Ru(1) C(111) C(121) . . . . 6(1) no O(2) Ru(1) C(120) C(110) . . . . -88.5(4) no O(2) Ru(1) C(121) C(111) . . . . -174(1) no O(2) C(4) C(3) C(2) . . . . -0.2(7) no O(3) Ru(1) O(1) C(2) . . . . -91.8(6) no O(3) Ru(1) O(2) C(4) . . . . 172.3(3) no O(3) Ru(1) O(4) C(9) . . . . -0.8(3) no O(3) Ru(1) N(1) C(13) . . . . -46.8(3) no O(3) Ru(1) N(1) C(17) . . . . 134.1(3) no O(3) Ru(1) C(110) C(120) . . . . 179.4(4) no O(3) Ru(1) C(111) C(121) . . . . 93(1) no O(3) Ru(1) C(120) C(110) . . . . -0.6(5) no O(3) Ru(1) C(121) C(111) . . . . -89(1) no O(3) C(7) C(8) C(9) . . . . 2.6(6) no O(4) Ru(1) O(1) C(2) . . . . -176.5(3) no O(4) Ru(1) O(2) C(4) . . . . 81(1) no O(4) Ru(1) O(3) C(7) . . . . 0.7(3) no O(4) Ru(1) N(1) C(13) . . . . -140.3(3) no O(4) Ru(1) N(1) C(17) . . . . 40.6(3) no O(4) Ru(1) C(110) C(120) . . . . -87.6(4) no O(4) Ru(1) C(111) C(121) . . . . -174(1) no O(4) Ru(1) C(120) C(110) . . . . 93.1(4) no O(4) Ru(1) C(121) C(111) . . . . 6(1) no O(4) C(9) C(8) C(7) . . . . -2.8(7) no N(1) Ru(1) O(1) C(2) . . . . -87.8(3) no N(1) Ru(1) O(2) C(4) . . . . 86.4(3) no N(1) Ru(1) O(3) C(7) . . . . -87.3(3) no N(1) Ru(1) O(4) C(9) . . . . 84.8(3) no N(1) Ru(1) C(110) C(120) . . . . -177.5(5) no N(1) Ru(1) C(111) C(121) . . . . 172(1) no N(1) Ru(1) C(120) C(110) . . . . 177.9(4) no N(1) Ru(1) C(121) C(111) . . . . -175.3(9) no N(1) C(13) C(14) C(15) . . . . -0.6(6) no N(1) C(17) C(16) C(15) . . . . 1.1(6) no C(1) C(2) C(3) C(4) . . . . -175.9(4) no C(2) O(1) Ru(1) C(110) . . . . 93.3(3) no C(2) O(1) Ru(1) C(111) . . . . 106.3(6) no C(2) O(1) Ru(1) C(120) . . . . 92.4(3) no C(2) O(1) Ru(1) C(121) . . . . 68.7(5) no C(2) C(3) C(4) C(5) . . . . 178.3(4) no C(4) O(2) Ru(1) C(110) . . . . -110.4(3) no C(4) O(2) Ru(1) C(111) . . . . -96.8(6) no C(4) O(2) Ru(1) C(120) . . . . -74.3(3) no C(4) O(2) Ru(1) C(121) . . . . -93.2(5) no C(6) C(7) C(8) C(9) . . . . -178.6(4) no C(7) O(3) Ru(1) C(110) . . . . 91.8(3) no C(7) O(3) Ru(1) C(111) . . . . 78.7(6) no C(7) O(3) Ru(1) C(120) . . . . 92.2(3) no C(7) O(3) Ru(1) C(121) . . . . 116.0(5) no C(7) C(8) C(9) C(10) . . . . 176.4(4) no C(9) O(4) Ru(1) C(110) . . . . -78.4(3) no C(9) O(4) Ru(1) C(111) . . . . -91.9(6) no C(9) O(4) Ru(1) C(120) . . . . -114.5(3) no C(9) O(4) Ru(1) C(121) . . . . -95.8(5) no C(13) N(1) Ru(1) C(110) . . . . -49.8(7) no C(13) N(1) Ru(1) C(111) . . . . -127(2) no C(13) N(1) Ru(1) C(120) . . . . 134.6(6) no C(13) N(1) Ru(1) C(121) . . . . 41(1) no C(13) N(1) C(17) C(16) . . . . -1.8(5) no C(13) C(14) C(15) C(16) . . . . -0.2(6) no C(14) C(13) N(1) C(17) . . . . 1.6(5) no C(14) C(15) C(16) C(17) . . . . 0.0(6) no C(17) N(1) Ru(1) C(110) . . . . 131.1(6) no C(17) N(1) Ru(1) C(111) . . . . 54(2) no C(17) N(1) Ru(1) C(120) . . . . -44.5(7) no C(17) N(1) Ru(1) C(121) . . . . -138(1) no #===END